Lacunary Wells-Dawson Sandwich Complexes - Synthesis, Characterization, and Stability Studies of Multi-Iron Species

Israel Martyr Mbomekalle; Bineta Keita; Louis Nadjo; Wade A. Neiwert; Lei Zhang; Kenneth I. Hardcastle; Craig L. Hill; Travis M. Anderson

Lacunary Wells-Dawson Sandwich Complexes - Synthesis, Characterization, and Stability Studies of Multi-Iron Species

Israel Martyr Mbomekalle, Bineta Keita, Louis Nadjo, Wade A. Neiwert, Lei Zhang, Kenneth I. Hardcastle, Craig L. Hill, Travis M. Anderson

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Abstract

Reaction of α-Na₁₂(As₂W₁₅O ₅₆) with Fe^II in 1 M NaCl solution followed by air oxidation yields αααα-H₂Na ₁₄[(NaOH₂)₂Fe^III₂-(As₂W₁₅O₅₆)₂] (Na2), the arsenic analogue of the divacant lacunary sandwich, ααα α-H₂Na₁₄[(NaOH₂)₂Fe ^III₂(P₂W₁₅O₅₆) ₂] (Na1). This complex (Na2) consists of a Na₂Fe ₂ central unit sandwiched between two B-α-As₂W ₁₅O₅₆^12- moieties. Both Na1 and Na2 react with one equivalent of Fe^III to give ααβα-Na ₁₄[(NaOH₂)(Fe^IIIOH₂)(Fe ^III)₂(X₂W₁₅O₅₆) ₂], where X = P (Na3) or As (Na4), or two equivalents of Mn ^II to give αββα-Na₁₄[(Mn ^IIOH₂)₂(Fe^III)₂(X ₂W₁₅O₅₆)₂], where X = P (Na5) or As (Na6). A single-crystal X-ray diffraction analysis of Na5 has been carried out [a = 13.5387(8) Å, b = 13.9327(9) Å, c = 21.3347(13) Å, α = 92.921(1) °, β = 94,367(1) °, γ = 118.154(1) °, triclinic, P1̄, R1 = 5.49%, based on 24662 independent reflections], which revealed a Mn₂Fe₂ central unit sandwiched between two B-α-P₂W₁₅O₅₆^12- units. All of the new complexes have been characterized by FTIR spectroscopy, UV/Visible spectroscopy, elemental analyses, and cyclic voltammetry, and they are all stable for at least 24 h over a wide pH range (0-7), except for Na4, which is unstable below pH 2.

Original language	English (US)
Pages (from-to)	3924-3928
Number of pages	5
Journal	European Journal of Inorganic Chemistry
Issue number	21
State	Published - Nov 7 2003

Keywords

Iron
Manganese
Polyoxometalates
Sandwich complexes

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Lacunary Wells-Dawson Sandwich Complexes - Synthesis, Characterization, and Stability Studies of Multi-Iron Species. / Mbomekalle, Israel Martyr; Keita, Bineta; Nadjo, Louis; Neiwert, Wade A.; Zhang, Lei; Hardcastle, Kenneth I.; Hill, Craig L.; Anderson, Travis M.

In: European Journal of Inorganic Chemistry, No. 21, 07.11.2003, p. 3924-3928.

Research output: Contribution to journal › Article › peer-review

@article{60b3771b81054b5daa291c14ea68570b,

title = "Lacunary Wells-Dawson Sandwich Complexes - Synthesis, Characterization, and Stability Studies of Multi-Iron Species",

abstract = "Reaction of α-Na12(As2W15O 56) with FeII in 1 M NaCl solution followed by air oxidation yields αααα-H2Na 14[(NaOH2)2FeIII2-(As2W15O56)2] (Na2), the arsenic analogue of the divacant lacunary sandwich, ααα α-H2Na14[(NaOH2)2Fe III2(P2W15O56) 2] (Na1). This complex (Na2) consists of a Na2Fe 2 central unit sandwiched between two B-α-As2W 15O5612- moieties. Both Na1 and Na2 react with one equivalent of FeIII to give ααβα-Na 14[(NaOH2)(FeIIIOH2)(Fe III)2(X2W15O56) 2], where X = P (Na3) or As (Na4), or two equivalents of Mn II to give αββα-Na14[(Mn IIOH2)2(FeIII)2(X 2W15O56)2], where X = P (Na5) or As (Na6). A single-crystal X-ray diffraction analysis of Na5 has been carried out [a = 13.5387(8) {\AA}, b = 13.9327(9) {\AA}, c = 21.3347(13) {\AA}, α = 92.921(1) °, β = 94,367(1) °, γ = 118.154(1) °, triclinic, P{\=1}, R1 = 5.49%, based on 24662 independent reflections], which revealed a Mn2Fe2 central unit sandwiched between two B-α-P2W15O5612- units. All of the new complexes have been characterized by FTIR spectroscopy, UV/Visible spectroscopy, elemental analyses, and cyclic voltammetry, and they are all stable for at least 24 h over a wide pH range (0-7), except for Na4, which is unstable below pH 2.",

keywords = "Iron, Manganese, Polyoxometalates, Sandwich complexes",

author = "Mbomekalle, {Israel Martyr} and Bineta Keita and Louis Nadjo and Neiwert, {Wade A.} and Lei Zhang and Hardcastle, {Kenneth I.} and Hill, {Craig L.} and Anderson, {Travis M.}",

year = "2003",

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language = "English (US)",

pages = "3924--3928",

journal = "Chemische Berichte",

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T1 - Lacunary Wells-Dawson Sandwich Complexes - Synthesis, Characterization, and Stability Studies of Multi-Iron Species

AU - Mbomekalle, Israel Martyr

AU - Keita, Bineta

AU - Nadjo, Louis

AU - Neiwert, Wade A.

AU - Zhang, Lei

AU - Hardcastle, Kenneth I.

AU - Hill, Craig L.

AU - Anderson, Travis M.

PY - 2003/11/7

Y1 - 2003/11/7

N2 - Reaction of α-Na12(As2W15O 56) with FeII in 1 M NaCl solution followed by air oxidation yields αααα-H2Na 14[(NaOH2)2FeIII2-(As2W15O56)2] (Na2), the arsenic analogue of the divacant lacunary sandwich, ααα α-H2Na14[(NaOH2)2Fe III2(P2W15O56) 2] (Na1). This complex (Na2) consists of a Na2Fe 2 central unit sandwiched between two B-α-As2W 15O5612- moieties. Both Na1 and Na2 react with one equivalent of FeIII to give ααβα-Na 14[(NaOH2)(FeIIIOH2)(Fe III)2(X2W15O56) 2], where X = P (Na3) or As (Na4), or two equivalents of Mn II to give αββα-Na14[(Mn IIOH2)2(FeIII)2(X 2W15O56)2], where X = P (Na5) or As (Na6). A single-crystal X-ray diffraction analysis of Na5 has been carried out [a = 13.5387(8) Å, b = 13.9327(9) Å, c = 21.3347(13) Å, α = 92.921(1) °, β = 94,367(1) °, γ = 118.154(1) °, triclinic, P1̄, R1 = 5.49%, based on 24662 independent reflections], which revealed a Mn2Fe2 central unit sandwiched between two B-α-P2W15O5612- units. All of the new complexes have been characterized by FTIR spectroscopy, UV/Visible spectroscopy, elemental analyses, and cyclic voltammetry, and they are all stable for at least 24 h over a wide pH range (0-7), except for Na4, which is unstable below pH 2.

AB - Reaction of α-Na12(As2W15O 56) with FeII in 1 M NaCl solution followed by air oxidation yields αααα-H2Na 14[(NaOH2)2FeIII2-(As2W15O56)2] (Na2), the arsenic analogue of the divacant lacunary sandwich, ααα α-H2Na14[(NaOH2)2Fe III2(P2W15O56) 2] (Na1). This complex (Na2) consists of a Na2Fe 2 central unit sandwiched between two B-α-As2W 15O5612- moieties. Both Na1 and Na2 react with one equivalent of FeIII to give ααβα-Na 14[(NaOH2)(FeIIIOH2)(Fe III)2(X2W15O56) 2], where X = P (Na3) or As (Na4), or two equivalents of Mn II to give αββα-Na14[(Mn IIOH2)2(FeIII)2(X 2W15O56)2], where X = P (Na5) or As (Na6). A single-crystal X-ray diffraction analysis of Na5 has been carried out [a = 13.5387(8) Å, b = 13.9327(9) Å, c = 21.3347(13) Å, α = 92.921(1) °, β = 94,367(1) °, γ = 118.154(1) °, triclinic, P1̄, R1 = 5.49%, based on 24662 independent reflections], which revealed a Mn2Fe2 central unit sandwiched between two B-α-P2W15O5612- units. All of the new complexes have been characterized by FTIR spectroscopy, UV/Visible spectroscopy, elemental analyses, and cyclic voltammetry, and they are all stable for at least 24 h over a wide pH range (0-7), except for Na4, which is unstable below pH 2.

KW - Iron

KW - Manganese

KW - Polyoxometalates

KW - Sandwich complexes

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